Process for the production of resinous materials.



C.GRANEL."

PROCESS-FOR THE PRODUCITION OF RESINOAUS MATERIALS.

' APPLICATION FILED APR. H. 1913.

Patlited Jul 11, 1916.

CAMILLE GRANEL, or BOUSCAT PAR LEsrERon, LANDES, FRANCE.

Specification of Letters Patent.

PROCESS FOR THE PRODUCTION OF RESINQUS MATERIALS.

Application filed A rn11,1s1a SerlalNo.-760,42.

To all whom it may concern:

Be it known that I, OAMILLE for'the'extraction of resinousmaterials-cons."

tained'in the residues of the distillation or purification of pinetappings or turpentine;

According to. this process, such resinous materials are extractedby'means of a suitable solvent such, for instance, as bisulfid ofcarbon, tetrachlorid of carbon, alcohols, benzols, petroleums, essentialoils, and the like, by operating in a manner similar to the usual onefor the extraction of grain or cake oils by the use of bisulfid ofcarbon, either continuously or discontinuously. By means of theapplication of such novel process of extraction to the treatment of thewaste or resinous residues, there can be recovered the'greater part ofthe resinous materials contained in the residues of the distillation ofpine-tappings; on treating the residues direct from the purification ofthese tappings there is obtained a much greater output of the drymaterials contained in the said residues with the production of pitch ofa brighter color.

One method of application of such process will now be described, by Wayof example, with reference to the accompanying diagrammatic drawings.

The resinous residues are placed in an extractor 1 between twoperforated plates 2'and 3 covered with filtering tissue or fabric. Theextractor being hermetically closed, there is forced through a conduit4:, by means of a pump 5, the solvent, either bisulfid of carbon orother solvent, from a closed vat 6. Such solvent rises through the massto be treated, dissolves the resinous materials and then passes througha conduit 7, to a filter 8, to separate from the charged solvents anyparticles of the residues carried along with it, and from the filter thecharged solvent is delivered to a still boiler 9 heated by a perforatedvessel or stirrer 10 and a serpentine steam pipe 11. The solvent whichis distilled passes for conden- 55 sation purposes to; a cooling vessel12,

GnA'NEL, a citizen of the Republic of France, -residing whence itreturns to the vat 6 through a con- I Patented July 11, 1916.

duit 13. Toward the close of the distillae tion, the last traces of. thesolvent are expelled by raising the temperature progres surely to 100?centigrade, and lastly a jet of steam ofa temperature of about 150centigrade is sent in direct, 'so as to expel "ntirely the solvent andthe Watercondensed in the mass, 1n order to obtain a'transparentproduct. What remains of the solvent in the extractor is then broughtback into the yet 6 through the conduit 14, provided'wih a cock115. Whendripping is over, steam'is .sent into the serpentine bubbler pipe 16located underneath the plate 2. Such steam,

passes through the exhausted residues and vaporizes the solvent withwhich they may still be impregnated; the mixture of vapors 1s condensedin the serpentine pipe 1'1,

whence a conduit 18 brings the mixtureof water and solvent back to thevat 6. The water lies at the top of the solvent and prevents theevaporation of the latter. Lastly, the exhausted residues areWithdrawn'from the extractor.

From time to time, the solvent' must be rectified, as it takes in littleby little an essential oil from the distillation of theresinoussolution. For that purpose, the rectitying liquid is sent into thedistillation chamber 9 and heated therein to a temperature comprisedbetween the boiling point of the solvent 'and that of the essential oil.The oil thus separated can then be freed of the traces of solvent whichit still contains by a treatment with chlorid of lime or any othersuitable treatment. Of course, this method of operation given by way ofexample can be modified without departing from the invention. Inparticular, the process may be the same as that used, for instance, inthe manufacture of oils for the continuousextraction by means ofbisulfid of carbon.

With solvents such as alcohols, benzols, petroleums, essential oils, andthe like the operations may be the same as with bisulfid If use is madeof alcohols, they must be rectified after each operation by well knownmeans.

It must be observed that resinous waste comprises several resinsunequally soluble in different solvents 'and that advantage may be takenof such difi'erences of solubility to obtain the division into fractionsof the resins which are present. In particular,

the residues include yellow resins called colophony, soluble in certainwell known solvents, and red or brown resins, insoluble in petroleums,for instance. If therefore it is desired, to extract only resins havingbut little color, all that need be done is to choose the solvent in thepetroleum and hydrocarbon series with but little benzin and to make thedissolution at a temperature be-. lowthe melting point of the coloringmaterials. For such purpose use may be made of a vacuum with advantage.

Claims:

1. A process for the extraction of the resinous materials contained inthe Waste from the distillation of the tappings, consisting in 'forcingthrough the mass of tapping waste a solvent from a closed reservoir,such solvent being so selected as to dissolve the clear resins While notacting on the darker .resin's in operating at a temperature below themelting point on the darker resins, in,

distilling the 'resinous solution thus obtained, in condensing thevapors given ofi',

and in returning the condensed liquor to the said closed reservoir. i

2. The herein described process of extracting resinous matter containedin the residues from the distillation of pine tappings, which consistsin treating said residues with a volatile solvent in a hermeti callysealed vessel, separating the solution in forcing under pressurecarbonbisulfid through the waste mass starting from a closed tub, saidmass being placed in anextractor, then in gathering said carbon bisulfidcharged With .resin dissolved-in a distilling boiler, in distilling saidresin carbon bisulfid in said boiler, in conducting the carbon bisulfidthrough a refrigerant, then in said closed tubalone, in causing thepassage of steam at a temperature of about. 150 C. through the resinmass in the boiler, in

, bringing back to said closed tub the greater part of theremainder ofcarbon bisulfid charged with resin in said extractor; in-

sending through the latter steam in order to remove the balance of thecarbon bisulfid, in

fid, and in bringing the products of said condensation into the saidclosed receptacle, substantially as described.

In testimony, that I claim the foregoing as my invention Ihave signed myname in presence of two-subscribing Witnesses;

- CAMILLE GRANEL.

Witnesses:' v

GILEVORISPEL,

' HENRY PHILLIPS.

.70 condensing said steam and the carbon bisul-

